Benzoyl Peroxide, Hydrous: Benzoylis Peroxidum Cum Aqua

EUROPEAN PHARMACOPOEIA 5.

0 Benzoyl peroxide, hydrous

B. Solution S (see Tests) gives reaction (a) of benzoates 01/2005:0704

(2.3.1).
BENZOYL PEROXIDE, HYDROUS
TESTS
Solution S. Dissolve 5.0 g in alcohol R and dilute to 100 ml Benzoylis peroxidum cum aqua
with the same solvent.
Appearance of solution. Solution S is clear (2.2.1) and
colourless (2.2.2, Method II).
Carbonisable substances. Dissolve 0.5 g with shaking in
5 ml of sulphuric acid R. After 5 min, the solution is not
more intensely coloured than reference solution Y5 (2.2.2,
Method I).
C14H10O4 Mr 242.2
Oxidisable substances. Dissolve 0.2 g in 10 ml of boiling
water R. Cool, shake and filter. To the filtrate add 1 ml of DEFINITION
dilute sulphuric acid R and 0.2 ml of 0.02 M potassium Content :
permanganate. After 5 min, the solution is still coloured
pink. dibenzoyl peroxide : 70.0 per cent to 77.0 per cent,
water : minimum 20.0 per cent.
Halogenated compounds and halides.
All glassware used must be chloride-free and may be CHARACTERS
prepared by soaking overnight in a 500 g/l solution of Appearance : white, amorphous or granular powder.
nitric acid R, rinsed with water R and stored full of water R. Solubility : practically insoluble in water, soluble in acetone,
It is recommended that glassware be reserved for this test. soluble in methylene chloride with the separation of water,
Solution (a). Dissolve 6.7 g of the substance to be examined slightly soluble in alcohol.
in a mixture of 40 ml of 1 M sodium hydroxide and 50 ml It loses water rapidly on exposure to air with a risk of
of alcohol R and dilute to 100.0 ml with water R. To 10.0 ml explosion.
of this solution add 7.5 ml of dilute sodium hydroxide Mix the entire sample thoroughly before carrying out the
solution R and 0.125 g of nickel-aluminium alloy R and following tests.
heat on a water-bath for 10 min. Allow to cool to room
temperature, filter into a 25 ml volumetric flask and wash IDENTIFICATION
with three quantities, each of 2 ml, of alcohol R. Dilute the
filtrate and washings to 25.0 ml with water R. This solution First identification : B
is used to prepare solution A. Second identification : A, C, D.
Solution (b). In the same manner, prepare a similar solution A. Dissolve 80.0 mg in alcohol R and dilute to 100.0 ml
without the substance to be examined. This solution is used with the same solvent. Dilute 10.0 ml of the solution
to prepare solution B. to 100.0 ml with alcohol R (solution A). Dilute 10.0 ml
of solution A to 100.0 ml with alcohol R (solution B).
In four 25 ml volumetric flasks, place separately 10 ml Examined between 250 nm and 300 nm (2.2.25),
of solution (a), 10 ml of solution (b), 10 ml of chloride solution A shows an absorption maximum at 274 nm and
standard solution (8 ppm Cl) R (used to prepare solution C) a shoulder at about 282 nm. Examined between 220 nm
and 10 ml of water R. To each flask add 5 ml of ferric and 250 nm, solution B shows an absorption maximum at
ammonium sulphate solution R5, mix and add dropwise 235 nm. The ratio of the absorbance at the maximum at
and with swirling 2 ml of nitric acid R and 5 ml of mercuric 235 nm (solution B) to that at the maximum at 274 nm
thiocyanate solution R. Shake. Dilute the contents of each (solution A) is 1.17 to 1.21.
flask to 25.0 ml with water R and allow the solutions to B. Infrared absorption spectrophotometry (2.2.24).
stand in a water-bath at 20 C for 15 min. Measure at 460 nm
the absorbance (2.2.25) of solution A using solution B as Comparison : Ph. Eur. reference spectrum of hydrous
the compensation liquid, and the absorbance of solution C benzoyl peroxide.
using the solution obtained with 10 ml of water R as the C. Dissolve about 25 mg in 2 ml of acetone R. Add 1 ml of a
compensation liquid. The absorbance of solution A is not 10 g/l solution of diethylphenylenediamine sulphate R
greater than that of solution C (300 ppm). and mix. A red colour develops which quickly darkens
Heavy metals (2.4.8). 12 ml of solution S complies with limit and becomes dark violet within 5 min.
test B for heavy metals (10 ppm). Prepare the standard using D. To 1 g add 5 ml of alcohol R, 5 ml of dilute sodium
a mixture of 5 ml of lead standard solution (1 ppm Pb) R hydroxide solution R and 10 ml of water R. Boil the
and 5 ml of alcohol R. mixture under reflux for 20 min. Cool. The solution gives
reaction (c) of benzoates (2.3.1).
Sulphated ash (2.4.14). Not more than 0.1 per cent,
determined on 1.0 g. TESTS
Acidity. Dissolve a quantity of the substance to be examined
ASSAY containing the equivalent of 1.0 g of dibenzoyl peroxide in
Dissolve 0.200 g in 20 ml of alcohol R and titrate with 0.1 M 25 ml of acetone R, add 75 ml of water R and filter. Wash
sodium hydroxide, using 0.1 ml of phenol red solution R as the residue with two quantities, each of 10 ml, of water R.
indicator, until the colour changes from yellow to violet-red. Combine the filtrate and the washings and add 0.25 ml of
phenolphthalein solution R1. Not more than 1.25 ml of
1 ml of 0.1 M sodium hydroxide is equivalent to 12.21 mg 0.1 M sodium hydroxide is required to change the colour of
of C7H6O2. the indicator. Carry out a blank test.
General Notices (1) apply to all monographs and other texts 1073
Benzoyl peroxide, hydrous EUROPEAN PHARMACOPOEIA 5.0
Related substances. Liquid chromatography (2.2.29). Chlorides (2.4.4) : maximum 0.4 per cent.
Prepare the solutions immediately before use. Dissolve a quantity of the substance to be examined
Test solution. Dissolve a quantity of the substance to be containing the equivalent of 0.5 g of dibenzoyl peroxide in
examined containing the equivalent of 0.10 g of dibenzoyl 15 ml of acetone R. Add, while stirring, 50 ml of 0.05 M
peroxide in acetonitrile R and dilute to 50 ml with the same nitric acid. Allow to stand for 10 min and filter. Wash the
solvent. residue with 2 quantities, each of 10 ml, of 0.05 M nitric
acid. Combine the filtrate and the washings and dilute to
Reference solution (a). Dilute 1.0 ml of the test solution to 100 ml with 0.05 M nitric acid. 2.5 ml of the solution diluted
100.0 ml with acetonitrile R. Dilute 1.0 ml of this solution to to 15.0 ml with water R complies with the limit test for
10.0 ml with acetonitrile R. chlorides.
Reference solution (b). Dissolve 30.0 mg of benzoic acid R
in the mobile phase and dilute to 100.0 ml with the mobile ASSAY
phase. Dilute 1.0 ml of the solution to 10.0 ml with the Solution (a). Dissolve 2.500 g immediately before use in
mobile phase. 75 ml of dimethylformamide R and dilute to 100.0 ml with
Reference solution (c). Dissolve 50.0 mg of ethyl benzoate R the same solvent.
in the mobile phase and dilute to 100.0 ml with the mobile Dibenzoyl peroxide. To 5.0 ml of solution (a) add 20 ml
phase. Dilute 1.0 ml of the solution to 100.0 ml with the of acetone R and 3 ml of a 500 g/l solution of potassium
mobile phase. iodide R and mix. Allow to stand for 1 min. Titrate with
0.1 M sodium thiosulphate using 1 ml of starch solution R,
Reference solution (d). Dissolve 50.0 mg of benzaldehyde R added towards the end of the titration, as indicator. Carry
in the mobile phase and dilute to 100.0 ml with the mobile out a blank titration.
phase. Dilute 1.0 ml of the solution to 100.0 ml with the
mobile phase. 1 ml of 0.1 M sodium thiosulphate is equivalent to 12.11 mg
of C14H10O4.
Reference solution (e). Dissolve 30.0 mg of benzoic acid R
and 30.0 mg of benzaldehyde R in the mobile phase and Water (2.5.12). Carry out the semi-micro determination
dilute to 100.0 ml with the mobile phase. Dilute 1.0 ml of the of water, using 5.0 ml of solution (a). Use as the solvent
solution to 10.0 ml with the mobile phase. a mixture of 20.0 ml of anhydrous methanol R and
3.0 ml of a 100 g/l solution of potassium iodide R in
Column : dimethylformamide R. After adding solution (a), stir for
size : l = 0.25 m, = 4.6 mm, 5 min before starting the titration. Carry out a blank
determination.
stationary phase: octadecylsilyl silica gel for Calculate the percentage content of water using the
chromatography R (10 m), expression :
Mobile phase : glacial acetic acid R, acetonitrile R, water R
(1:500:500 V/V/V).
Flow rate : 1 ml/min.
Detection : spectrophotometer at 235 nm. n1 = number of millilitres of iodosulphurous reagent R
used in the sample determination,
Injection : 20 l loop injector. n2 = number of millilitres of iodosulphurous reagent R
Run time : 2 times the retention time of dibenzoyl peroxide. used in the blank determination,
Relative retention with reference to dibenzoyl peroxide w = water equivalent of iodosulphurous reagent R in
(retention time = about 28.4 min) : impurity B = about 0.15 ; milligrams of water per millilitre of reagent,
impurity A = about 0.2 ; impurity C = about 0.4. m = mass of the substance to be examined used for
System suitability : reference solution (e) : the preparation of solution (a) in grams,
resolution : minimum 6 between the peaks corresponding p = percentage content of dibenzoyl peroxide.
to benzoic acid and benzaldehyde.
STORAGE
Limits :
In a container that has been treated to reduce static
impurity A : not more than the area of the principal peak discharge and that has a device for release of excess pressure,
in the chromatogram obtained with reference solution (d) at a temperature of 2 C to 8 C, protected from light.
(0.25 per cent),
impurity B : not more than the area of the principal peak IMPURITIES
in the chromatogram obtained with reference solution (b)
(1.5 per cent),
impurity C : not more than the area of the principal peak
in the chromatogram obtained with reference solution (c)
(0.25 per cent),
any other impurity : not more than the area of the
principal peak in the chromatogram obtained with A. R = H : benzaldehyde,
reference solution (a) (0.1 per cent),
disregard limit : 0.2 times the area of the principal peak B. R = OH : benzoic acid,
in the chromatogram obtained with reference solution (a)
(0.02 per cent). C. R = O-CH2-CH3 : ethyl benzoate.
1074 See the information section on general monographs (cover pages)

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EUROPEAN PHARMACOPOEIA 5.

0 Benzoyl peroxide, hydrous

B. Solution S (see Tests) gives reaction (a) of benzoates 01/2005:0704

1074 See the information section on general monographs (cover pages)

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